Reclaiming distillation residues



July l0, 1928.

S. P. COLEMAN ET AL RECLAIMING DISTILLATION RESIDUES v Filed Feb. '7, 1924 ...o 22MB ZO. PDJOw. O ZmIPncQZ @ma @HW @5M an 10 templated. tank in laterally staggered order so as to 60 Patented .iuly 10,1928. y 1,676,687

UNITEDTSTATES PATENT oFFICE.

STEWART I. COLEMAN, OF CAMBRIDGE, MASSACHUSETTS, AN'J) WAYNE S. '.lElUGrHES,v

OF GOOSE CREEK, TEXAS, ASSIGNORS TO STANDARD 1 DEVELOPMENT COMPANY, A CORPORATION OF DELAWARE. l

RECLAHNG DISTILLATION RESIDUES.

Application filed February 7, 1924. Serial No. 691,162.

This invention relates to the art of reand an apron 8 to prevent currents at the. claiming distillation residues and more parpoint of discharge into the tank. The setticularly such residues as are left in redistling tank may vary considerably in its tilling lubricating stocks which contain forni and dimension, but an advantageous naphthenic compounds. The invention will layout is illustrated in the drawing in that 55 be understood from the following descripit is so arranged as to conserve space andtion taken in connection withv the accomyet accomplish a feasible stratification of panying drawing which represents an isothe ingredients of the residue. To this end metric view of one'form of apparatus conthe battles 9,' 10 and 11 are-arranged in the There lubricating stocks containing compel the contained liquids to travel very naphthenic acids are redistilled-in `the presslowly and free from turbulence to the reence of caustic soda 'or other sodium comspective points of discharge. Valveconpound, a heavy residue comprising an vintrolled draw-oil pipes 12 and 13 are ar- 15 timate mixture of sodium naphthenate or ranged at the bottom of the tank, and from 65 other naphthenates and high viscosity oil a point near its top a draw-olf pipe 14 is left in the still. Heretofore such resileads to discharge into a second tank 15. dues have been thought useful only for Along the bottom of the second tanka suitadmix'ture with fuel oil. In accordance able heatingmeans isarranged, illustrated with the present invention, however, We are in the drawing, for instance, as a steam 70 enabled to reclaim such residues and decoil 16. A valve-controlled draw-oli pipe rive therefrom a lubricating oil stock of 17 is provided at'thebottom of this tank u higher viscosity and desirable vproperties and an adjustable swing draw-oit- .pipe 18 otherwise, and also naphthenic compounds at the top.

.25 which are capable of various uses. 1 A current of water being provided in the 75 In carrying out the invention We take thetrough by the Water inlet pipe 2, the distillaf residue, preferably as it is drawn hot from vtion residue is discharged gently upon the the still, and flour it upon a ,moving stream surface of the Water through the pipe 4, and of water. The velocity of the water-stream the liowing" waterv and .supernatant'oily should not be such as to cause turbulence or residuum is passed along into the settling 80 mixing, but on the contrary is advisablypf tank-where a stratification into layers takes such gentle character that the oily residue place,.the lower layer consisting of water discharged/thereon may quietly spread out and dissolved naphthenates. On coming in over its surfaceand be carried alongwithcontact with the water, the water-soluble i out risk of emulsilication. advantanaphthenates rapidly dissolve out from the S5 geous formA of apparatus for the .practicing oily mixture and go into the water'. At of this rocess is represented in the drawthe start sufficient water is primarily suping in w 'ch the reference numeral 1 desigplied to the tank to bring the level up well nates a trough Ihaving at itsend a means, tothe top and after the feed of residuum is 40 for a supply of water, illustrated as a pipe established and stratification into layers has 90 2 with control valve 3. Further along in taken placethe lower layer is drawn olf at the trough is a 'discharge means for a dissuch a rate as to allow an adequate accumutillation residue, illustrated as .a pipe 4 lat-ion of the upper layers, permitting suit- With control valve 5, the pipe preferably able draW-oif thereof into the second tank having a spray-head or slotted-head disl5. By proper regulation ofthe draw-ott 95 charge 4so as to' effect as thorough a spread valves the process may thus be made to funcl 'of the residue upon the water surface as tion in continuous manner, the stratificafeasible. The trough discharges into a ysettion levels being maintained at relatively tlingr tank 6, a dam 7 being provided to constant points. The oil layer and some4 maintain a fixed Water level in the trough, naphthenic compounds pass over to the 100 second tank, and here final stratification and separation allows of the withdrawing of the clean oil from the top, the swing pipe 18 by its vertical adju'stability allowing 'of the taking olf of the oil only. From the bottom of the tank the naphthenic compounds, occurring here chiefly as naphthenates of the heavy metals, especially iron, are withdrawn for further treatment. This treatment may vary somewhat, butpreferably would comprise the subjecting of the naphthenate mixture, it being in the form of emulsion, to the action of sulphuric acid. This serves to decompose the naphthenates and setfree the naphthenicacid and the emulsified oil, and on settling, these constituent-s can be drawn off from the top and the sludge be run to waste.

It will be understood, however, that the aphthenates of the heavy metal form such a minor component of the distillation residue vthat in many cases itl is not worth while attempting a separate separation and treatment o these, but the separation may proceed along the main lines of division of the oil on the one hand and the'water-soluble naphthenates on the other. The watersoluble naphthenates may be recovered from the water by salting out -or'by concentration, and these compounds are'then lavailable for various uses as desired.

If preferred, the stratification levels can be so maintained th'at the heavy lmetal emulsilied naphthenic layer may be drawn o' vfrom tank 6 and further separated, as mentioned in the foregoing, instead of being carried over into tank 15 and thence being se arated off; that is, the recise point at w ich' the separation of t e heavy metal emulsied naphthenate layer occurs. is a matter of cho1ce in operating detail.

What we claim is:

1. The process of reclaiming naphthenic'A I layer, subjecting the residual material to further stratification, withdrawing the oil from the top and withdrawing the water containing metal naphthenates from the bottom layer.

2. The process of reclaiming naphthenic A distillation residues, which comprises discharging'the hot residue onto the surface of 'flowing water, then allowing stratification into layers to occur, ,withdrawing the water A and dissolved naphthenate from the bottom layer. and withdrawing the oil from the top.

3. The process of reclaiming naphthenic distillation residues, `which comprises dis-- charging the residue onto the1si1rface of gently moving water, then retardin'g-'I the flow and allowing stratification 1 int layers to occur, and separately withdrawing the water and dissolved naphthenate from the.

bottom layer and the oil from thetop.

4. The process of reclaiming naphthemc distillation residues; which comprises discharging the 'residue onto the surface of Y, :A

moving water, and allowingt stratification into layers andseparately withdrawing the water and' dissolved na hthenate 'ing one layer and the oilv in the ot er.

' STEWART P. ,COLEMA' WAYNE S. HUGHES. 

